CN115349613A - Preparation method of rosa roxburghii biological freeze-dried preparation - Google Patents
Preparation method of rosa roxburghii biological freeze-dried preparation Download PDFInfo
- Publication number
- CN115349613A CN115349613A CN202210737030.5A CN202210737030A CN115349613A CN 115349613 A CN115349613 A CN 115349613A CN 202210737030 A CN202210737030 A CN 202210737030A CN 115349613 A CN115349613 A CN 115349613A
- Authority
- CN
- China
- Prior art keywords
- roxburgh rose
- dried
- freeze
- preparation
- vacuum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 130
- 240000002547 Rosa roxburghii Species 0.000 title claims abstract description 54
- 235000000640 Rosa roxburghii Nutrition 0.000 title claims abstract description 54
- 241000220317 Rosa Species 0.000 claims abstract description 232
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 125
- 238000001035 drying Methods 0.000 claims abstract description 119
- 239000000463 material Substances 0.000 claims abstract description 95
- 230000001954 sterilising effect Effects 0.000 claims abstract description 87
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 69
- 238000002061 vacuum sublimation Methods 0.000 claims abstract description 59
- 238000007710 freezing Methods 0.000 claims abstract description 46
- 230000008014 freezing Effects 0.000 claims abstract description 42
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 34
- 229930003944 flavone Natural products 0.000 claims abstract description 34
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 34
- 235000011949 flavones Nutrition 0.000 claims abstract description 34
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 238000003795 desorption Methods 0.000 claims abstract description 19
- 239000003826 tablet Substances 0.000 claims description 77
- 238000004458 analytical method Methods 0.000 claims description 72
- 239000004033 plastic Substances 0.000 claims description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 65
- 238000000034 method Methods 0.000 claims description 56
- 239000008187 granular material Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 35
- 238000004140 cleaning Methods 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 29
- 235000013399 edible fruits Nutrition 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 25
- 238000004806 packaging method and process Methods 0.000 claims description 25
- 238000000859 sublimation Methods 0.000 claims description 23
- 230000008022 sublimation Effects 0.000 claims description 23
- 239000011248 coating agent Substances 0.000 claims description 21
- 230000000249 desinfective effect Effects 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 15
- 239000002775 capsule Substances 0.000 claims description 13
- 238000011282 treatment Methods 0.000 claims description 12
- 244000052616 bacterial pathogen Species 0.000 claims description 11
- 239000010720 hydraulic oil Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 239000004375 Dextrin Substances 0.000 claims description 9
- 229920001353 Dextrin Polymers 0.000 claims description 9
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 9
- 241000607142 Salmonella Species 0.000 claims description 9
- 241000607768 Shigella Species 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 241000191967 Staphylococcus aureus Species 0.000 claims description 9
- 235000019425 dextrin Nutrition 0.000 claims description 9
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 9
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 9
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 9
- 230000004071 biological effect Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 239000002352 surface water Substances 0.000 claims description 6
- 102000019197 Superoxide Dismutase Human genes 0.000 abstract description 99
- 108010012715 Superoxide dismutase Proteins 0.000 abstract description 99
- 230000000694 effects Effects 0.000 abstract description 24
- 238000001727 in vivo Methods 0.000 abstract description 10
- 102000004190 Enzymes Human genes 0.000 abstract description 6
- 108090000790 Enzymes Proteins 0.000 abstract description 6
- 235000015097 nutrients Nutrition 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 118
- 239000003570 air Substances 0.000 description 44
- 238000002474 experimental method Methods 0.000 description 24
- 230000008569 process Effects 0.000 description 23
- 238000010521 absorption reaction Methods 0.000 description 21
- 238000005469 granulation Methods 0.000 description 13
- 230000003179 granulation Effects 0.000 description 13
- 239000003094 microcapsule Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 238000001514 detection method Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 11
- 230000002265 prevention Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000009455 aseptic packaging Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 206010028980 Neoplasm Diseases 0.000 description 8
- 230000032683 aging Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- 238000004108 freeze drying Methods 0.000 description 7
- 239000008176 lyophilized powder Substances 0.000 description 7
- 229920001277 pectin Polymers 0.000 description 7
- 239000001814 pectin Substances 0.000 description 7
- 235000010987 pectin Nutrition 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 201000011510 cancer Diseases 0.000 description 6
- 230000003749 cleanliness Effects 0.000 description 6
- 230000006378 damage Effects 0.000 description 6
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 6
- 238000007908 dry granulation Methods 0.000 description 6
- 230000006870 function Effects 0.000 description 6
- 238000011835 investigation Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 235000016709 nutrition Nutrition 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 201000010099 disease Diseases 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- -1 superoxide anions Chemical class 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 108091005804 Peptidases Proteins 0.000 description 4
- 239000004365 Protease Substances 0.000 description 4
- 235000014443 Pyrus communis Nutrition 0.000 description 4
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000011162 core material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000005243 fluidization Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 230000036039 immunity Effects 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 210000003097 mucus Anatomy 0.000 description 4
- 238000007619 statistical method Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 3
- 238000009395 breeding Methods 0.000 description 3
- 230000001488 breeding effect Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- 238000012858 packaging process Methods 0.000 description 3
- 230000000144 pharmacologic effect Effects 0.000 description 3
- 239000003223 protective agent Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000009777 vacuum freeze-drying Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- PJVXUVWGSCCGHT-ZPYZYFCMSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;(3s,4r,5r)-1,3,4,5,6-pentahydroxyhexan-2-one Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O.OC[C@@H](O)[C@@H](O)[C@H](O)C(=O)CO PJVXUVWGSCCGHT-ZPYZYFCMSA-N 0.000 description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 208000023275 Autoimmune disease Diseases 0.000 description 2
- 208000017667 Chronic Disease Diseases 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 102000052575 Proto-Oncogene Human genes 0.000 description 2
- 108700020978 Proto-Oncogene Proteins 0.000 description 2
- 235000004789 Rosa xanthina Nutrition 0.000 description 2
- 238000000692 Student's t-test Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003796 beauty Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000002542 deteriorative effect Effects 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 125000004073 flavone group Chemical group 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 235000013402 health food Nutrition 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 235000021581 juice product Nutrition 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000000050 nutritive effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229960002477 riboflavin Drugs 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 239000006188 syrup Substances 0.000 description 2
- 235000020357 syrup Nutrition 0.000 description 2
- 238000012353 t test Methods 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 229960003495 thiamine Drugs 0.000 description 2
- 125000003287 1H-imidazol-4-ylmethyl group Chemical group [H]N1C([H])=NC(C([H])([H])[*])=C1[H] 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 102000016938 Catalase Human genes 0.000 description 1
- 108010053835 Catalase Proteins 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000004367 Lipase Substances 0.000 description 1
- 102000004882 Lipase Human genes 0.000 description 1
- 108090001060 Lipase Proteins 0.000 description 1
- 244000151018 Maranta arundinacea Species 0.000 description 1
- 235000010804 Maranta arundinacea Nutrition 0.000 description 1
- 229920000715 Mucilage Polymers 0.000 description 1
- 241000158764 Murraya Species 0.000 description 1
- 102000043276 Oncogene Human genes 0.000 description 1
- 108700020796 Oncogene Proteins 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000011449 Rosa Nutrition 0.000 description 1
- 241000109329 Rosa xanthina Species 0.000 description 1
- 241000220222 Rosaceae Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 235000012419 Thalia geniculata Nutrition 0.000 description 1
- JZRWCGZRTZMZEH-UHFFFAOYSA-N Thiamine Natural products CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N JZRWCGZRTZMZEH-UHFFFAOYSA-N 0.000 description 1
- 102000044209 Tumor Suppressor Genes Human genes 0.000 description 1
- 108700025716 Tumor Suppressor Genes Proteins 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 229930003451 Vitamin B1 Natural products 0.000 description 1
- 206010047601 Vitamin B1 deficiency Diseases 0.000 description 1
- 229930003471 Vitamin B2 Natural products 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 206010047623 Vitamin C deficiency Diseases 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 208000002894 beriberi Diseases 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000001185 bone marrow Anatomy 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000001055 chewing effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000003394 haemopoietic effect Effects 0.000 description 1
- 210000005260 human cell Anatomy 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 235000008935 nutritious Nutrition 0.000 description 1
- 230000004768 organ dysfunction Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000019612 pigmentation Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000004252 protein component Nutrition 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000019192 riboflavin Nutrition 0.000 description 1
- 239000002151 riboflavin Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 208000010233 scurvy Diseases 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 208000019116 sleep disease Diseases 0.000 description 1
- 208000020685 sleep-wake disease Diseases 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 235000019157 thiamine Nutrition 0.000 description 1
- KYMBYSLLVAOCFI-UHFFFAOYSA-N thiamine Chemical compound CC1=C(CCO)SCN1CC1=CN=C(C)N=C1N KYMBYSLLVAOCFI-UHFFFAOYSA-N 0.000 description 1
- 239000011721 thiamine Substances 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000019164 vitamin B2 Nutrition 0.000 description 1
- 239000011716 vitamin B2 Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/01—Instant products; Powders; Flakes; Granules
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/015—Preserving by irradiation or electric treatment without heating effect
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/015—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with pressure variation, shock, acceleration or shear stress or cavitation
- A23L3/0155—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with pressure variation, shock, acceleration or shear stress or cavitation using sub- or super-atmospheric pressures, or pressure variations transmitted by a liquid or gas
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/738—Rosa (rose)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/02—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
- A61K47/38—Cellulose; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/0005—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts
- A61L2/0011—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor for pharmaceuticals, biologicals or living parts using physical methods
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/18—Antioxidants, e.g. antiradicals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2202/00—Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
- A61L2202/20—Targets to be treated
- A61L2202/21—Pharmaceuticals, e.g. medicaments, artificial body parts
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Food Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Nutrition Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Biochemistry (AREA)
- Mycology (AREA)
- Dermatology (AREA)
- Dispersion Chemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Toxicology (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a preparation method of a roxburgh rose biological freeze-dried preparation, which comprises the following steps: non-thermal sterilization (HPP) of fructus Rosae Normalis pure juice by using ultrahigh pressure container + ) And (2) processing, namely rapidly freezing the sterile roxburgh rose pure juice, carrying out vacuum sublimation drying and vacuum desorption drying in sequence at low temperature, mixing with auxiliary materials, and further processing according to actual conditions to prepare the required preparation. The biological freeze-dried preparation of the rosa roxburghii tratt has high content of superoxide dismutase (SOD) enzyme activity, VC and total flavone, has good stability, furthest reserves the nutrient components and the nutrient value of fresh rosa roxburghii tratt, is moisture-proof, convenient to carry and convenient to eat, can maintain the content level of SOD in vivo, and has good market prospect.
Description
Technical Field
The invention belongs to the technical field of biological food processing, and particularly relates to a preparation method of a roxburgh rose biological freeze-dried preparation.
Background
Roxburgh rose is a perennial deciduous shrub of Rosa of Rosaceae, and is commonly called Roxburgh rose, also called King fruit of mountain, senchu, arrowroot and Murraya. In summer and autumn, the fruits are mostly flat and spherical, the fruit meat is crisp, and the fruits have strong fragrance after being mature. The fructus Rosae Normalis is nutritious, and contains SOD, VC, VP1, VP2, VB1, VB2, VB-sitosterol, VE, VA, VD, VK, calcium, phosphorus, iron, tannin, fructus Rosae Normalis triterpene, lipase, fructus Rosae Normalis flavone, dietary fiber and microelements such as selenium and zinc. Wherein SOD, VC and flavone are the most important contents of plants. Roxburgh rose is known as "the king of SOD" and "the king of vitamin C", is known as "magic pear" and "life-prolonging fruit" by folk, and is known as "nutrition bank".
SOD is considered to be the most magical enzyme in life science and technology. SOD is one of substances with the functions of anti-aging, immunoregulation, blood fat regulation, radiation resistance and beauty treatment, and is numbered as ECl.15.1.1 by the legal number; CAS [905489]1.SOD is one of the most important enzymes in the human body, and can delay aging because of its ability to scavenge free radicals. People are aged, and the aging signs are gradually seen, such as pigmentation and physical decline, because oxidation is generated in the body, and the supplement of antioxidants helps to reduce the oxidation speed and slow down the aging steps. Preventing and treating autoimmune diseases, and SOD has certain curative effect on various autoimmune diseases. The medical report indicates that the decline period of the antioxidant capacity is advanced to about 40 years old, and the light dependence on vegetables and fruits is not enough to eliminate the oxidation pressure formed by the inside and the outside of the human body. The prevention of chronic diseases, free radicals are the main causes of various chronic diseases and aging discovered by scientists, so that the free radicals are the source of 'ten thousand diseases' and are large enemies of human health, and the damage of the free radicals to the human body is accumulated day by day. In order to keep the body healthy and the oxidation speed slow, the SOD in the body needs to be kept sufficient; unfortunately, after 25 years old, the activity and concentration of SOD in human body are gradually reduced, so we must supplement exogenous SOD to make up for the missing SOD in human body, so that the human body will be healthy.
The detection shows that fresh fruit and original juice (without sterilization or heating sterilization) of the roxburgh rose contain 3 SOD, and the proportion of the three enzymes is as follows: the first 65.3%; the second 14.4%; and the third 20.3 percent. Compared with a compound preparation for treating diseases such as cancer and the like, resisting aging and beautifying, the roxburgh rose has the following functions: 1. enhancing body resistance, enhancing immunity, resisting virus, and preventing diseases. SOD in the roxburgh rose has obvious effects of relieving fatigue, improving immunity, supplementing energy and the like. 2. And (3) cancer prevention and resistance: the fructus Rosae Normalis is rich in superoxide dismutase (SOD) 10000U/ml. SOD is an active substance which is internationally recognized to have the effect of cancer prevention, and in addition, SOD has obvious effects on improving immunity, resisting radiation and the like and is the first killer of active oxygen free radicals which are the source of all diseases. The causes of tumors are numerous, but whatever the cause of the induced tumor, it is finally caused by the destruction of oncogenes by free radicals and the activation of proto-oncogenes. After SOD enters human cells, DNA can be protected, and self-repair is carried out at the same time, so that cancer suppressor genes and protooncogenes in the human body are stable and balanced, the hematopoietic function of bone marrow is improved, the immunity of the organism is stimulated and improved, cells which tend to mutate are damaged before canceration, and are prevented from dissociating to other parts of the body, and the purposes of cancer prevention and cancer resistance are achieved. Vitamin E, B-sitosterol, SOD and catalase in the roxburgh rose constitute a protection system for eliminating active oxygen such as free radicals of superoxide anions and the like, and the roxburgh rose has cancer prevention and anticancer effects. 3. And (4) resisting aging. SOD is an internationally recognized anti-aging drug. Fructus Rosae Normalis contains abundant superoxide dismutase (SOD), and its juice (non-sterilized or non-heated sterilized) can improve SOD activity, reduce Lipid Peroxide (LPO), and has anti-aging effect. SOD also has the effect of repairing damaged cells, so that the cell activity is greatly enhanced. SOD has the effect of eliminating free radicals of human body! 4. Has tranquilizing effect and can make people fall asleep quickly. SOD is used for clinically treating insomnia, can eliminate excessive free radicals in vivo, and can improve and treat tissue organ dysfunction and disorder, thereby achieving the purpose of treating sleep disorder. In addition, fructus Rosae Normalis also contains nutritional elements such as VC, vitamin B1 (thiamine acid), vitamin B2 (riboflavin), etc., and has effects of resisting oxidation, caring skin, removing lead, treating scurvy, treating beriberi, invigorating spleen, promoting digestion, relieving pain, reducing blood pressure, blood lipid, and preventing and treating diabetes.
At present, there are some documents on freeze-drying rosa roxburghii tratt to prepare instant food, such as:
1. the application number CN202110915141.6 discloses a roxburgh rose freeze-dried powder and a processing method thereof, wherein the roxburgh rose freeze-dried powder comprises roxburgh rose stock solution and fructose-glucose syrup, the first technical step is that roxburgh rose is squeezed to obtain juice after washing and drying control of roxburgh rose fruits to obtain roxburgh rose stock solution, and the roxburgh rose stock solution and the fructose-glucose syrup are mixed in proportion to obtain mixed solution; step two, putting the mixed solution into a quick-freezing warehouse for speed control, wherein the freezing temperature is-40 to-35 ℃; and step three, transferring the frozen mixed solution into a vacuum freeze dryer for vacuum drying to obtain a semi-finished product, wherein the vacuum degree is less than or equal to 100pa, and heating to promote drying in a vacuum environment, wherein the heating temperature is 30-55 ℃. The method freezes at-40 to-35 ℃, freezes all water such as free water in the mixed solution into solid state, quickly dries under high vacuum, the boiling point of water can be changed under vacuum environment, so that the solid ice in the raw material can be sublimated at low temperature and transformed into gas state, thereby drying the water, and keeping the color, shape, taste and the like of the raw material to the maximum extent, and most importantly, keeping the active ingredients of the raw material. However, the subsequent process of humidity control and product moisture prevention is not adopted in the scheme, and the roxburgh rose contains hydrophilic components such as sugar, starch, resin, pectin, mucus, mixed fluid, inorganic salt and the like, so that the freeze-dried product is very easy to absorb moisture, and becomes soft, caked, deliquesced and even liquefied due to moisture absorption, thereby mildewing, breeding bacteria, deteriorating and being unsafe to eat. In addition, the scheme also does not adopt a sterilization process, the raw materials are operated in a non-clean area, the pollution is certain, the bacteria breeding inside the raw materials is also certain after the raw materials are placed for a long time and absorb moisture, and the quality cannot be guaranteed. Thus, shelf life is short, commercial poor and unsafe.
2. Application number 201610354549X discloses a vacuum freeze-drying treatment process for Rosa roxburghii, which comprises the steps of (4) increasing the vacuum degree of a vacuum drying chamber to 100-150 pa, controlling the temperature to 70-80 ℃, and maintaining for 6-10 hours. SOD has biological activity for biological protease, SOD biological protease in the roxburgh rose is easily inactivated when the temperature is higher than 60 ℃, the temperature is controlled to be 70-80 ℃, the SOD is kept for 6-10 hours, most SOD is inactivated, VC and flavone are largely destroyed, and the due value of the SOD is lost.
3. Application No. CN201510774934.5 discloses a production method of a seedless roxburgh rose freeze-dried tablet, which comprises the following steps: a. raw material treatment: cleaning fresh seedless roxburgh rose, slicing and airing surface moisture; b. Freezing; c. and (3) vacuum drying: controlling the vacuum degree in the vacuum freeze dryer to be 20-40 Pa, the drying temperature to be-25 to-18 ℃, and controlling the drying time to be 3-6 h; d. and (3) resolving and drying: gradually reducing the vacuum degree in the vacuum freeze dryer to 5-10 Pa, gradually increasing the drying temperature to 35-50 ℃, and drying for 5-15 min to obtain the seedless roxburgh rose freeze-dried slices; e. aseptic packaging; the freeze-dried seedless roxburgh rose slices produced by the method can keep the original flavor and form, the loss of nutrients and functional components is avoided, the freeze-dried seedless roxburgh rose slices conform to the regulations in the edible fungi sanitary standard GB7096-2003, and the water content index is lower than 1/2 of the national standard. However, this solution has the following disadvantages: (1) whether the rosa roxburghii tratt is a rosa roxburghii tratt with seeds or a rosa roxburghii tratt without seeds, the rosa roxburghii tratt is divided into an edible part and a non-edible part, the edible part is mainly pulp, the non-edible part is mainly pericarp and seeds, if juicing is carried out, the juice yield is about 50 percent generally, namely, a great part of rosa roxburghii tratt is inedible. (2) According to the scheme, a peeling process is not adopted before slicing, the seedless roxburgh roses with the diameters of 3-8cm are selected according to the first embodiment and the second embodiment, after slicing, the minimum diameter of the finished product freeze-dried seedless roxburgh rose slices can be 0.5cm, and the eating method is only chewing. Although the freeze-dried slices are not frozen into powder through the freeze-drying process, the non-edible insoluble long fibers in the peel are still wrapped around the freeze-dried slices, and the insoluble long fibers cannot be swallowed after being chewed, so that the product quality is influenced. (3) The technical scheme has no humidity control process, although in the second and third embodiments, e and packaging: the dried product is taken out in time, but has a certain time difference in industrial production. Moreover, the rosa roxburghii contains hydrophilic components such as saccharides, starch, resin, pectin, mucus, mixture, inorganic salt and the like, has strong hygroscopicity, is easy to absorb moisture in the air, and is difficult to ensure the quality of the freeze-dried rosa roxburghii slices under the working condition. (4) Although the technical scheme is aseptic packaging, no sterilization process is adopted, and the quality of the freeze-dried seedless roxburgh rose slices is difficult to ensure under the working condition.
4. Patent application 201610464953.2 discloses a preparation method of freeze-dried particles of fructus Rosae Normalis, and further, the invention provides a preparation method of freeze-dried particles of fructus Rosae Normalis, which can also have the following characteristics: the method comprises the following specific steps: (a), standing the raw juice of the roxburgh rose for at least 5h, and filtering; (b) vacuum concentrating to 1/4-1/5 of the original volume; (c) Adding a protective agent into the concentrated solution, stirring until the protective agent is completely dissolved, and adjusting the pH value to 6-8 after filtering; (d) carrying out a vacuum freeze drying process; (e) And crushing, and then carrying out aseptic packaging to obtain the roxburgh rose freeze-dried particles. Wherein in step (e), the comminuting and the aseptic packaging are both carried out in an environment having a temperature not exceeding 25 ℃ and a relative air humidity not exceeding 40%. And sealing by adopting an aluminum-plastic composite bag to obtain the roxburgh rose freeze-dried particles. However, the technical solution has the following disadvantages and shortcomings: (1) the Rosa roxburghii normal juice is static in the air for 5 hours, VC, SOD, flavone, etc. are oxidized, and the content is reduced. (2) In a non-clean area, the rosa roxburghii tratt juice is still in the air for 5 hours, the juice is polluted, a sterilization process is not adopted, and the freeze-dried product cannot ensure the product quality although the crushing and the packaging are carried out in a sterile room. (3) Although the protective agent is added into the concentrated solution, the glucose can prevent the solution from caking during drying, so that the dried product is loose and fragile. However, the roxburgh rose contains hydrophilic components such as sugar, starch, resin, pectin, mucilage, mixture and inorganic salt, has strong hygroscopicity and viscosity, and is poor in fluidity, lubricity and formability.
The rosa roxburghii tratt has short storage period, contains more tannin, has heavy bitter taste and is difficult to accept; the roxburgh rose contains rich superoxide dismutase (SOD) and the like as bioactive protease, for example, juicing, sterilization is needed for prolonging the shelf life of the roxburgh rose, the traditional heating sterilization can destroy the bioactivity of the SOD and the like in the roxburgh rose to lose the due value of the SOD, and other nutritional ingredients such as VC, ketones and the like can be damaged. When the roxburgh rose pure juice is prepared into the freeze-dried product, the roxburgh rose pure juice freeze-dried product contains strong physiological activity and chemical components with definite pharmacological action, and also contains hydrophilic components such as polysaccharide, pectin, mucus and the like, so that the roxburgh rose pure juice freeze-dried product has strong hygroscopicity, and the freeze-dried product becomes soft, blocks, deliquesces, mildews, breeds bacteria and even liquefies due to moisture absorption, thereby influencing the pharmacological and health-care values of the roxburgh rose pure juice freeze-dried product. Meanwhile, superoxide dismutase (SOD) has a short half-life in vivo, and its content in vivo should be maintained for a long period of time except for a few times of administration or eating.
The unique nutritive value of fresh roxburgh rose fruits in fruit and vegetable foods is important for human health, aging resistance and beauty, but the prior art does not overcome the defects of high-temperature sterilization or non-sterilization and moisture-proof technologies of roxburgh rose freeze-dried preparations or products, and cannot research a roxburgh rose freeze-dried product which can retain the nutritional ingredients and the medical value of the roxburgh rose freeze-dried preparations or products to the maximum extent, is moisture-proof, convenient to carry and eat and can maintain the content level of SOD in vivo.
Disclosure of Invention
Aiming at the problems and the defects of the prior art, the invention provides a preparation method of a roxburgh rose biological freeze-dried preparation. The application is characterized in that the roxburgh rose pure juice is subjected to non-thermal sterilization, is lyophilized and mixed with auxiliary materials, and is further processed into a required preparation according to actual conditions to obtain the roxburgh rose biological freeze-dried preparation, the content of VC and flavone in the roxburgh rose biological freeze-dried preparation is low, the stability is good, the activity of superoxide dismutase (SOD) enzyme is not damaged, even the activity of the SOD enzyme is improved or activated, the nutritional ingredients and the nutritional value of fresh roxburgh rose fruits are retained to the maximum extent, and the product is moisture-proof, convenient to carry and convenient to eat, can maintain the content level of SOD in vivo for a long time, and has a good market prospect.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing biological lyophilized preparation of fructus Rosae Normalis comprises: carrying out non-thermal sterilization treatment on the roxburgh rose pure juice by adopting ultrahigh pressure (HPP +), quickly freezing the sterile roxburgh rose pure juice, carrying out vacuum sublimation drying and vacuum desorption drying treatment in sequence in a low-temperature environment, mixing the roxburgh rose pure juice with auxiliary materials to obtain a mixed material, and further processing the mixed material into required tablets, granules, powder or capsules according to actual conditions to obtain the roxburgh rose biological freeze-dried preparation.
Further, the granules are prepared by granulating, microencapsulating and aseptically packaging the mixed materials; the tablet is prepared by granulating, tabletting, coating, aluminum-plastic bubble cap or aseptic bagging or bottling the mixture.
The micro-encapsulation is a micro-capsule which is prepared by granulating a mixed material, namely a capsule core material, by using a natural or synthetic polymer film-forming material, namely a capsule material, and then embedding the granulated mixed material, namely the capsule core material to form a semi-permeable or sealed capsule film with the diameter of 5-250 mu m.
The processes of granulation, microencapsulation, coating, packaging and the like mainly have the moisture-proof function, so that the product is prevented from absorbing moisture and deteriorating; the slow release process of biological freeze dried roxburgh rose preparation includes microcapsule embedding or microcapsule encapsulating. The microcapsule has moisture-proof and slow-release effects to maintain SOD content in vivo.
Further, the preparation method of the rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh rosa roxburghii tratt fruits and air-drying the fresh rosa roxburghii tratt fruits to remove surface moisture for later use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice;
(3) Non-heat sterilization (HPP +) treatment: sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an UHP, HHP or HPP ultrahigh-pressure container, adding a medium, then sealing a high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice;
(4) Cleaning and disinfecting a large package: conveying the sterilized roxburgh rose pure juice large package obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, sterilizing and disinfecting; the big package is a plastic soft package or is filled in a plastic bottle;
(5) Quick freezing: in an aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose juice into a bracket layering tray, and sending into a quick-freezing warehouse or a freeze-drying machine for quick freezing to obtain frozen roxburgh rose juice;
(6) Vacuum sublimation drying: conveying the frozen pure roxburgh rose support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried pure roxburgh rose product, namely a vacuum sublimation dried product;
(7) And (3) vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material;
(8) Mixing: according to the weight portion ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed, and further processing into the required preparation according to actual conditions to obtain the biological freeze-dried preparation of the roxburgh rose.
Further, in the step (2), the filter screen for the first filtration is 200-300 meshes, and the filter screen for the second filtration is 400-800 meshes.
The filtering aims to remove ineffective components such as cellulose, pectin and the like in the juice and reduce the yield of freeze-dried roxburgh rose juice, and the yield of the freeze-dried powder with the water content of 10 percent is less than or equal to 5 percent, so that the content of the effective components of the freeze-dried powder is improved, the defect of large dosage is overcome, and the hygroscopicity of freeze-dried products is reduced.
Further, in the step (3), the medium is water or high-grade hydraulic oil; when the medium in the ultrahigh pressure container is water, applying pressure of 400-600 MPa to the roxburgh rose pure juice packaged by the plastic flexible package or the plastic bottle, and keeping the pressure for 5-15 min; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying pressure of 100-1000 MPa to the roxburgh rose pure juice packaged by the plastic flexible package or the plastic bottle; the pressure maintaining time is 1-30 min.
The application adopts ultra-high-pressure sterilization technology (UHP for short) or high-static pressure technology (HHP for short) or high-pressure sterilization technology (HPP for short) to carry out non-thermal sterilization, because the non-thermal sterilization (HPP +) can kill bacteria, moulds and yeasts in the plastic soft package or plastic bottle packaged pure roxburgh rose juice, and active ingredients such as SOD, VC, VP and the like in the plastic soft package or plastic bottle packaged pure roxburgh rose juice can not be greatly inactivated like high-temperature sterilization.
Further, in step (5), the temperature of the quick freezing is-30 to-40 ℃.
Further, in the step (6), the vacuum degree of the vacuum sublimation drying is 30-150 pa, the temperature is 30-40 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%.
Further, in the step (7), the vacuum degree of the vacuum analysis drying is 5-30 pa, the temperature is 40-60 ℃, the relative humidity of air is 20-40%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of = (0.3-0.4): 0.2-0.4), and the mass ratio of the microcrystalline cellulose, the micro-powder silica gel and the dextrin is 1.
The auxiliary material has the effects of moisture absorption prevention, lubrication, slow release and the like, the auxiliary material is added to ensure that the technological process of the biological freeze-dried preparation of the roxburgh rose is smoothly carried out and the safety and the effectiveness of a finished product are ensured, the auxiliary material has good fluidity, hygroscopicity, formability and lubricity, can be a single auxiliary material or a combined auxiliary material, and the drug loading of the auxiliary material is not lower than the self weight.
The door of the sublimation drying chamber is communicated with the non-humidity control area sterile room or the clean area, and the rest is isolated from the non-humidity control area sterile room; the sterilized roxburgh rose pure juice is quickly frozen at the temperature of minus 30 to minus 40 ℃, and then frozen water molecules are directly sublimated into water vapor at the temperature of 30 to 40 ℃ in a vacuum environment of 30 to 150pa to be removed, so that a freeze-dried roxburgh rose pure juice freeze-dried product with the water content of 10 +/-2 percent is obtained.
Further, in step (8), the mass ratio of the vacuum-analyzed dried product to the dry auxiliary material =1 x, and x is not more than 1.
During vacuum analysis and drying, the sublimation freeze-dried product and the auxiliary materials are put in a vacuum environment of 5-30 pa, and a part of water remained in the sublimation freeze-dried product is evaporated at the temperature of 40-60 ℃ so that the water content of the sublimation freeze-dried product reaches the requirement of 5 +/-2%. The vacuum analysis drying chamber and the chamber communicated with the vacuum analysis drying chamber are subjected to humidity control treatment, the relative humidity of air is controlled to be 20-40%, the door of the vacuum analysis drying chamber is communicated with the humidity control area in a sterile manner, and the rest of the vacuum analysis drying chamber is isolated from the humidity control area in the sterile manner; the air pressure of the sterile room in the humidity control area is more than 5pa greater than that of the sterile room in the non-humidity control area.
Further, when the biological freeze-dried roxburgh rose preparation is a granule, the mixture is prepared by granulation, microencapsulation and aseptic packaging; when the biological freeze-dried roxburgh rose preparation is a tablet, the mixture is prepared by granulation, tabletting, coating, aluminum-plastic bubble cap or aseptic bag packaging or bottled packaging; the rotating speed is 500-600 r/min. When the fluidized coating method is adopted for coating, the fluidization temperature is less than or equal to 60 ℃.
The granulation adopts dry granulation: the freeze-dried product and auxiliary materials are uniformly mixed, then are pressed into slices with certain hardness and diameter by a tablet machine, and then are crushed into freeze-dried preparations with certain particle size by a particle crusher, and the method comprises the steps of rolling, granule finishing and the like. The steps of mixing the vacuum-resolved dried product with the auxiliary material and dry granulation can be carried out in one piece of equipment.
The microcapsule is encapsulated, namely microencapsulation, and is characterized in that a natural or synthetic high polymer film-forming material, namely a capsule wall material, is utilized to granulate freeze-dried products of the roxburgh rose, namely a capsule core material, and then the freeze-dried products are encapsulated to form a semi-permeable or sealed capsule film and a micro capsule with the diameter of 5-250 mu m by using a certain method and equipment; the microcapsule has moisture-proof and slow-release effects to maintain SOD content in vivo.
The tabletting is to granulate the freeze-dried roxburgh rose product and the mixture thereof or encapsulate the granulated microcapsules, namely microencapsulation, and then to carry out tabletting by adopting a rotary multi-punching technology. The tablet is packaged by aluminum plastic blister, i.e. the freeze-dried preparation of the roxburgh rose after being coated is packaged by a blister packaging machine, and simultaneously has the functions of printing and printing.
The coating is to coat the freeze-dried roxburgh rose preparation after tabletting by adopting a rolling or fluidized coating method. When the fluidized coating method is adopted for coating, the hot air temperature is less than or equal to 60 ℃, and the activity of superoxide dismutase SOD can be damaged when the hot air temperature is higher than 60 ℃. The fluidization temperature is less than or equal to 60 ℃ during coating.
Adopting a dry granulation technology: the roxburgh rose freeze-dried powder is fine powder, so that the specific surface area is large, and the moisture absorption capacity is strong; after dry granulation, larger particles are formed, the specific surface area is reduced, and the hygroscopicity is reduced. By adopting the microcapsule embedding or microencapsulation technology, the freeze-dried preparation, namely the capsule core is coated by natural or synthetic capsule wall materials to form a semi-permeable or totally-enclosed membrane which can effectively prevent the freeze-dried roxburgh rose preparation from absorbing moisture. The tabletting freeze-dried roxburgh rose preparation adopts a coating technology to coat the formed freeze-dried roxburgh rose preparation, so that the moisture absorption of the freeze-dried roxburgh rose preparation is effectively prevented. The coated freeze-dried roxburgh rose preparation is subjected to blister packaging or particle vacuum packaging, so that the phenomenon that the roxburgh rose preparation is completely opened and is contacted with air to absorb moisture when the roxburgh rose preparation is eaten or taken can be avoided.
Furthermore, the content of VC in the biological freeze-dried preparation of the roxburgh rose is more than or equal to 30mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g. Pathogenic bacteria, namely salmonella, shigella and staphylococcus aureus, are not detected in the roxburgh rose biological freeze-dried preparation; the critical relative humidity of the roxburgh rose biological freeze-dried preparation is more than or equal to 70 percent. The quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent. The biological freeze-dried preparation of the rosa roxburghii tratt prepared by the application meets the requirements.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand.
The large package cleaning, disinfecting, quick freezing and vacuum sublimation drying processes are carried out in a sterile room or a clean area non-humidity control area, the cleaning level is not lower than 30 ten thousand levels, the relative humidity is 40-65%, the non-clean area and the clean area are isolated by a clean air curtain, and the air pressure of the clean area is more than 5pa greater than that of the non-clean area; vacuum desorption drying, mixing a vacuum desorption dried product with auxiliary materials, granulating, embedding or microencapsulating microcapsules, tabletting, coating, tablet aluminum plastic bubble caps or aseptic bagging or bottling packaging and aseptic packaging of granules are carried out in a humidity control area, the relative humidity is 20-40%, the humidity control area and a non-humidity control area are separated and blocked by a clean air curtain, and the air pressure of the humidity control area is more than 5pa greater than that of the non-humidity control area; the uncleaned area and the outdoor are separated by an air curtain, and the air pressure of the uncleaned area is more than 10pa greater than the outdoor air pressure; and in the humidity control area in the sterile or clean area, the relative air humidity is 20-40%.
The preparation process also comprises boxing, labeling and warehousing, namely, the packaged freeze-dried roxburgh rose preparation is subjected to boxing, labeling and warehousing.
In the whole production process, the air pressure of the sterile clean area is 5pa greater than that of the non-clean area; the unclean section air pressure is 105pa greater than the outdoor ambient air pressure.
In the application, fresh roxburgh rose fruits are cleaned, air-dried, juiced, sterilized by non-heat (HPP +), boxed and labeled and packaged in a non-clean area; cleaning and disinfecting a large package, freezing in a quick freezing warehouse, and drying in a vacuum sublimation way in a non-humidity-control area in a sterile room or a clean area, wherein the clean level is not lower than 30 ten thousand levels, and the relative humidity of the non-humidity-control area is 40-65%; vacuum desorption drying together with auxiliary materials, mixing with the auxiliary materials, dry granulation, microcapsule embedding or microencapsulation, tabletting, coating, tablet aluminum plastic bubble cap or aseptic bag packaging or bottle packaging and granule aseptic packaging are carried out in an aseptic area or a clean area humidity control area, and the relative air humidity is 20-40%.
The quick freezing, the vacuum sublimation drying and the vacuum desorption drying can be carried out in one freeze dryer. The vacuum sublimation drying and the vacuum desorption drying can be carried out in one freeze dryer. The door of the quick freezing warehouse is communicated with the sterile room or the clean area, and the rest is isolated from the sterile room. The quick freezing can be carried out in a freeze-drying box in a freeze dryer or a special quick-freezing warehouse; the mixing with the auxiliary materials and the dry granulation step may be carried out in one apparatus.
The door of the sublimation drying chamber is communicated with the non-humidity control area sterile room or the clean area, and the rest is isolated from the non-humidity control area sterile room; the door of the analysis drying chamber is communicated with the aseptic chamber of the humidity control area, and the rest of the analysis drying chamber is isolated from the aseptic chamber of the humidity control area; the sterile room of the humidity control area and the sterile room of the non-humidity control area are isolated by a clean air curtain; the air pressure of the sterile room in the humidity control area is more than 5pa greater than that of the sterile room in the non-humidity control area; the air pressure of the sterile room is more than 10pa greater than the air pressure of the non-sterile environment; the unclean region is separated from the outdoor by an air curtain. When the fluidized coating method is adopted for coating, the temperature of hot air is less than or equal to 60 ℃, and the activity of superoxide dismutase SOD can be damaged when the temperature is higher than 60 ℃, so the temperature is controlled well.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) According to the application, after the roxburgh rose juice is freshly squeezed, a filter with a 400-800-mesh filter screen is used for secondary filtration, so that ineffective components such as cellulose, pectin, mucus and mixed juice in the juice are removed, the yield of the roxburgh rose juice after freeze drying is reduced, the yield of freeze-dried powder with the water content of 10% is less than or equal to 5%, the content of the effective components of the freeze-dried powder is improved, the defect of large administration dosage is overcome, and the hygroscopicity of freeze-dried products is reduced.
(2) The method adopts non-thermal (HPP +) sterilization and vacuum freeze-drying modes, can keep the activity of SOD biological protease in the freeze-dried roxburgh rose product, ensures that VC, flavone and the like in the freeze-dried roxburgh rose preparation are slightly damaged, and thus the nutritive value of the roxburgh rose is kept; meanwhile, the roxburgh rose is convenient to carry and eat, and plays a due role in preventing and treating diseases, protecting health, resisting aging, beautifying and the like.
(3) The freeze-dried roxburgh rose preparation contains hydrophilic components such as polysaccharide, pectin, mucoid and the like, has strong hygroscopicity, and influences the pharmacological and health-care values of the freeze-dried roxburgh rose preparation due to softening, caking, deliquescence, mildewing, bacteria breeding and even liquefaction caused by the hygroscopicity. In the preparation process, relevant key steps are carried out in the environment with the relative humidity of 20-40%, and the moisture absorption prevention technology is adopted in the preparation process by combining the preparation types, so that the influence on the product quality due to the fact that the process environment humidity is too high and the moisture absorption of the roxburgh rose freeze-dried preparation is caused is avoided. In addition, the technology of microcapsule embedding or microencapsulation and coating can not only effectively prevent moisture absorption, but also has slow release function, and because the half-life period of superoxide dismutase SOD in vivo is short, the freeze-dried roxburgh rose preparation can continuously and slowly release high-content SOD through microencapsulation and coating, so as to maintain a certain content level of SOD in vivo, thereby achieving the purposes of treatment and health care.
(4) The application is fast frozen, sublimation is dry, analysis is dry to be accomplished by the all-in-one generally. The yield of freeze-dried roxburgh rose juice is generally less than 5 percent, if an all-in-one machine is adopted, the quick freezing needs 8 to 12 hours, and the sublimation drying needs 6 to 10 hours, if the mass production is adopted, the production efficiency is influenced; sublimation drying and desorption drying are generally completed by an all-in-one machine, but because the yield of freeze-dried roxburgh rose pure juice is generally less than 5%, the consumption of the roxburgh rose pure juice is large, tray loading and unloading are long, the contact time of a freeze-dried preparation and air is long, and moisture absorption is inevitable, so that the product quality is influenced. Therefore, the three procedures of quick freezing, sublimation drying and analysis drying are separated in the process flow, and the analysis drying procedure is carried out in the humidity control area, so that the influence on the product quality caused by long time consumption for loading and unloading the tray and long moisture absorption time is avoided, and the production efficiency is improved.
(5) The existing production process flows of traditional Chinese medicine solid preparations such as tablets, capsules, granules and the like do not have processes of sterilizing and disinfecting raw materials, and although the processes of extracting, purifying, concentrating, drying and the like can be carried out in a clean area, the traditional Chinese medicine raw materials can be bacteria-carrying, so that the safety risk is brought to finished medicines. The roxburgh rose biological freeze-dried preparation adopts HPP + non-thermal sterilization and sterilization pretreatment, so that pathogenic bacteria (salmonella, shigella and staphylococcus aureus) cannot be detected, and the risk is avoided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the implementation examples or the description of the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some examples of the present invention, and that other drawings can be obtained by those skilled in the art without inventive step:
FIG. 1 is a flow chart of the process of the biological freeze-dried preparation of Rosa roxburghii Tratt of the present application;
FIG. 2 is a graph of Critical Relative Humidity (CRH) measured for coated tablets of a biologically lyophilized preparation of Rosa roxburghii Tratt according to the present application;
FIG. 3 is a graph of Critical Relative Humidity (CRH) determined for uncoated tablets of a lyophilized biological preparation of Rosa roxburghii of the present application;
fig. 4 is a graph of Critical Relative Humidity (CRH) measured for biologically lyophilized formulations of rosa roxburghii tratt granules of the present application.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A preparation method of a Rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice; the filter screen for the first filtration is 300 meshes, the filter screen for the second filtration is 600 meshes, and the yield of the freeze-dried powder with the water content of 10 percent is about 5 percent;
(3) Non-heat sterilization (HPP +): filling and sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an HPP ultrahigh-pressure container, adding medium water, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice; applying 600MPa pressure to the fructus Rosae Normalis pure juice packaged in plastic flexible package or plastic bottle, and keeping the pressure for 5min;
(4) Cleaning and disinfecting a large package: conveying the sterilized roxburgh rose pure juice large package obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, sterilizing and disinfecting;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose pure juice into bracket layered trays, and sending the tray into a quick freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature for quick freezing is-35 ℃;
(6) Vacuum sublimation drying: conveying the frozen pure roxburgh rose support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried pure roxburgh rose product, namely a vacuum sublimation dried product; the vacuum degree of the vacuum sublimation drying is 50pa, the temperature is 35 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material; the vacuum degree of the vacuum analysis drying is 10pa, the temperature is 50 ℃, the relative humidity of air is 20%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary material is a mixed auxiliary material prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of = 0.3.
(8) Mixing: according to the weight part ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed, and performing granulation, tabletting, coating and aluminum-plastic bubble cap packaging processes to obtain the roxburgh rose biological freeze-dried preparation which is an aluminum-plastic bubble cap packaging coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material is 1; the roxburgh rose biological freeze-dried preparation is a coated tablet; the rotating speed is 600r/min; the content of VC in the biological freeze-dried preparation of the roxburgh rose is more than or equal to 30mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) cannot be detected; the critical relative humidity of the obtained rosa roxburghii biological freeze-dried preparation is more than or equal to 70 percent, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand; the fluidization temperature is less than or equal to 60 ℃ during coating; and in the humidity control area in the sterile or clean area, the relative air humidity is 20-40%.
Example 2
A preparation method of a Rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice; the filter screen for the first filtration is 300 meshes, and the filter screen for the second filtration is 800 meshes;
(3) Non-heat sterilization (HPP +): filling and sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice; applying pressure of 500MPa to fructus Rosae Normalis pure juice packaged in plastic flexible package or plastic bottle, and keeping the pressure for 20min;
(4) Cleaning and disinfecting a large package: conveying the sterilized roxburgh rose pure juice large package obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, sterilizing and disinfecting;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose pure juice into bracket layered trays, and sending the tray into a quick freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature for quick freezing is-40 ℃;
(6) Vacuum sublimation drying: conveying the frozen roxburgh rose pure juice support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried roxburgh rose pure juice product, namely a vacuum sublimation dried product; the vacuum degree of the vacuum sublimation drying is 100pa, the temperature is 40 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material; the vacuum degree of the vacuum analysis drying is 20pa, the temperature is 45 ℃, the relative humidity of air is 40%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary material is a mixed auxiliary material prepared by mixing microcrystalline cellulose, aerosil and dextrin according to the mass ratio = 0.4.
(8) Mixing: mixing the vacuum-analyzed dried product and the dry auxiliary materials at a certain rotating speed, stirring, mixing, homogenizing, granulating, tabletting, and packaging in aseptic bags to obtain the fructus Rosae Normalis biological lyophilized preparation which is an aseptic bagged non-coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material = 1; the Rosa roxburghii biological freeze-dried preparation is a non-coated tablet; the rotating speed is 520r/min; the content of VC in the biological freeze-dried preparation of the roxburgh rose is more than or equal to 33mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 22000-55000 u/g, and the content of flavone is more than or equal to 4.4mg/g.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand; a humidity control area in an aseptic area or a clean area, wherein the relative humidity of air is 20-40%; the critical relative humidity of the obtained rosa roxburghii biological freeze-dried preparation is more than or equal to 70 percent, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent.
Example 3
A preparation method of a Rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice; the filter screen for the first filtration is 200 meshes, and the filter screen for the second filtration is 800 meshes;
(3) Non-thermal sterilization (HPP +): filling and sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 100MPa pressure to the roxburgh rose pure juice packaged by the plastic flexible package or the plastic bottle; maintaining the pressure for 30min;
(4) Cleaning and disinfecting a large package: conveying the large package of the sterile roxburgh rose juice obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose pure juice into bracket layered trays, and sending the tray into a quick freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature for quick freezing is-30 ℃;
(6) Vacuum sublimation drying: conveying the frozen roxburgh rose pure juice support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried roxburgh rose pure juice product, namely a vacuum sublimation dried product; the vacuum degree of the vacuum sublimation drying is 150pa, the temperature is 30 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material; the vacuum degree of the vacuum analysis drying is 30pa, the temperature is 40 ℃, the relative humidity of air is 30%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary material is a mixed auxiliary material prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of = 0.35.
(8) Mixing: according to the weight portion ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the dry auxiliary materials at a certain rotating speed, and performing granulation, microencapsulation and aseptic packaging processes to obtain the roxburgh rose biological freeze-dried preparation which is an aseptic packaged granule; the mass ratio of the vacuum analysis dried product to the drying auxiliary material = 1; the roxburgh rose biological freeze-dried preparation is sterile packaged granules; the rotating speed is 500r/min; the content of VC in the roxburgh rose biological freeze-dried preparation granules is more than or equal to 31.5mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 21000-52000 u/g, and the content of flavone is more than or equal to 4.2mg/g; the critical relative humidity of the obtained rosa roxburghii biological freeze-dried preparation is more than or equal to 70 percent, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand; and in the humidity control area in the sterile or clean area, the relative air humidity is 20-40%.
Example 4
A preparation method of a Rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice; the filter screen for the first filtration is 300 meshes, and the filter screen for the second filtration is 400 meshes;
(3) Non-heat sterilization (HPP +): filling and sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying 1000MPa pressure to the roxburgh rose pure juice packaged by the plastic flexible package or the plastic bottle; keeping the pressure for 1min;
(4) Cleaning and disinfecting a large package: conveying the large package of the sterile roxburgh rose juice obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, disinfection and sterilization;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose pure juice into bracket layered trays, and sending the tray into a quick freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice; the temperature for quick freezing is-40 ℃;
(6) Vacuum sublimation drying: conveying the frozen pure roxburgh rose support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried pure roxburgh rose product, namely a vacuum sublimation dried product; the vacuum degree of the vacuum sublimation drying is 30pa, the temperature is 40 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material; the vacuum degree of the vacuum analysis drying is 5pa, the temperature is 60 ℃, the relative humidity of air is 35%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary material is a mixed auxiliary material prepared by mixing microcrystalline cellulose, aerosil and dextrin according to the mass ratio = 0.25.
(8) Mixing: according to the weight portion ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the dried auxiliary materials at a certain rotating speed, and performing granulation, tabletting, coating and bottled packaging processes to obtain the roxburgh rose biological freeze-dried preparation which is a bottled and coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material = 1.7; the roxburgh rose biological freeze-dried preparation is a coated tablet; the rotating speed is 580r/min; the content of VC in the biological freeze-dried preparation of the roxburgh rose is more than or equal to 35mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 23000-58000/g, and the content of flavone is more than or equal to 4.7mg/g; the critical relative humidity of the obtained rosa roxburghii biological freeze-dried preparation is more than or equal to 70 percent, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand; the fluidization temperature of the coating is less than or equal to 60 ℃; a humidity control area in a sterile or clean area, wherein the relative humidity of air is 20-40%; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) were not detected.
Example 5
A preparation method of a Rosa roxburghii biological freeze-dried preparation comprises the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice; the filter screen for the first filtration is 250 meshes, and the filter screen for the second filtration is 700 meshes;
(3) Non-heat sterilization (HPP +): filling and sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an UHP, HHP or HPP ultrahigh-pressure container, adding medium high-grade hydraulic oil, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice; when the medium in the ultrahigh-pressure container is high-grade hydraulic oil, applying 500MPa pressure to the roxburgh rose pure juice packaged in the plastic flexible package or the plastic bottle; the pressure maintaining time is 15min;
(4) Cleaning and disinfecting a large package: conveying the sterilized roxburgh rose pure juice large package obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, sterilizing and disinfecting;
(5) Quick freezing: in an aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose juice into a bracket layering tray, and sending into a quick-freezing warehouse or a freeze-drying machine for quick freezing to obtain frozen roxburgh rose juice; the temperature for quick freezing is-35 ℃;
(6) Vacuum sublimation drying: conveying the frozen pure roxburgh rose support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried pure roxburgh rose product, namely a vacuum sublimation dried product; the vacuum degree of the vacuum sublimation drying is 90pa, the temperature is 35 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material; the vacuum degree of the vacuum analysis drying is 25pa, the temperature is 50 ℃, the relative humidity of air is 30%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary material is a mixed auxiliary material prepared by mixing microcrystalline cellulose, aerosil and dextrin according to the mass ratio = 0.3.
(8) Mixing: according to the weight part ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the drying auxiliary materials at a certain rotating speed, and performing granulation, tabletting and aluminum-plastic blister packaging processes to obtain the roxburgh rose biological freeze-dried preparation which is an aluminum-plastic blister packaging non-coated tablet; the mass ratio of the vacuum analysis dried product to the drying auxiliary material = 1; the Rosa roxburghii biological freeze-dried preparation is a non-coated tablet; the rotating speed is 550r/min; the content of VC in the biological freeze-dried preparation of the roxburgh rose is more than or equal to 30mg/g, the content of biological activity of SOD (superoxide dismutase) is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; the critical relative humidity of the obtained rosa roxburghii biological freeze-dried preparation is more than or equal to 70 percent, and the quality guarantee period is 18 months under the environment with the relative humidity of 60-75 percent.
Further, the cleanliness level of the sterile environment is not lower than 30 ten thousand; a humidity control area in an aseptic area or a clean area, wherein the relative humidity of air is 20-40%; pathogenic bacteria (salmonella, shigella, staphylococcus aureus) were not detected.
In order to verify the creativity of the technical scheme of the invention and the advancement of the comparison with the disclosed prior art, the following experiments are carried out:
comparative example 1
The difference from the example 1 is that: a method for preparing biological freeze-dried preparation of Rosa roxburghii Tratt comprises sterilizing at high temperature, namely heating fresh Rosa roxburghii Tratt juice to 75-90 deg.C for 15-16 s, and then aseptically packaging, wherein other conditions are not changed.
To further illustrate that the present invention can achieve the technical effects, the following experiments were performed:
experiment one:
the content of the main components of the roxburgh rose pure juice non-thermal sterilization analysis dry product and the freeze-dried preparation thereof is determined.
1. Purpose of the test
The main component content of the freeze-dried roxburgh rose preparation is changed after the dry product of the analysis of the pure roxburgh rose juice and auxiliary materials are mixed and are prepared by processes such as granulation and the like.
2. Test materials
2.1 test article
2.1.1 analysis-dried product of fructus Rosae Normalis pure juice
According to the method of the embodiment 1, the roxburgh rose is subjected to juicing, filtering, non-thermal sterilization, large-package cleaning and disinfection, quick freezing, vacuum sublimation drying and vacuum desorption drying processes to obtain a desorption dried product.
2.1.2 Rosa roxburghii biological freeze-drying preparation;
according to the method of the embodiment 1, the non-heat sterilized roxburgh rose pure juice desorption dry product or freeze-dried powder is mixed with auxiliary materials, the mass ratio of the desorption dry product to the auxiliary materials is 1.
2.2 Experimental groups
Taking 12 parts of fructus Rosae Normalis pure juice, resolving and drying, and numbering 2 g/part as control group.
12 parts of roxburgh rose biological agent, 3 tablets per part and 0.6g per tablet are taken as investigation groups and numbered respectively.
3. Experimental method
3.1VC (ascorbic acid) detection method: GB 5009.86-2016 (second method)
3.2SOD (superoxide dismutase) detection method: CTC-VM-007-2012
3.3 flavone detection method: total Flavonoids in chapter four of 2003 edition of health food inspection and evaluation
3.4 evaluation index
Respectively detecting the contents of VC, SOD and flavone in the dried product of fructus Rosae Normalis juice and fructus Rosae Normalis biological preparation.
As the mass ratio of the analysis dry product of the pure roxburgh rose juice to the auxiliary materials is 1.
3.5 Committee of the Integrated detection center of the national institute of inspection and quarantine
Report number CAIQS002100391300607.
4. Statistical analysis
The statistical software "clinician statistical assistant V10.0" was used, the experimental data were expressed as means ± SD, and statistical analysis was performed on each index by t-test of mean of two samples between groups, with p × < 0.05, p × < 0.01, p × 0.001, and the significance was poor.
5. Results of the experiment
The experimental results are shown in table 1 below.
TABLE 1VC, SOD, flavone control group and investigation group detection data
Note: the data of the control group is 1/2 of the actual detection data.
TABLE 2 average number of VC, SOD and flavone groups
As can be seen from Table 2, the contents of VC, SOD and flavone in the control group are respectively reduced by 1.84%, 1.14% and 2.79% compared with the investigation group, and the p values are all larger than 0.05, and the differences of the contents of VC, SOD and flavone in the control group and the investigation group, namely the contents of VC, SOD and flavone in the analysis dried product of the roxburgh rose pure juice are not significant compared with the roxburgh rose biological preparation, namely, the roxburgh rose biological freeze-dried preparation obtained by mixing the roxburgh rose pure juice analysis dried product with auxiliary materials and carrying out processes of granulation, tabletting, coating, packaging and the like has small damage degree on VC, SOD and flavone and has no significant difference between the VC, SOD and flavone.
Experiment two:
and (4) performing an experiment of destroying main nutrient components of the raw juice of the rosa roxburghii tratt by heating sterilization and non-heating sterilization.
1. Purpose of the experiment
And (4) inspecting the damage of the main nutrient components of the roxburgh rose juice by heat sterilization and non-heat sterilization.
2. Test materials
2.1 test article
TABLE 3 fresh fructus Rosae Normalis juice of the same batch
2.2 Experimental groups
2.2.1 according to the fresh roxburgh rose juice, adopting high-temperature sterilization and non-thermal sterilization to obtain pure roxburgh rose juice, dividing into 3 groups, wherein each group is 12 parts and numbered respectively.
2.2.2 1 group of fresh juice of fructus Rosae Normalis was used as control group, and 2 and 3 groups were used as investigation group.
3. Experimental methods
3.1VC (ascorbic acid) detection method GB 5009.86-2016 (second method).
3.2SOD (superoxide dismutase) detection method: according to CTC-VM-007-2012.
3.3 flavone detection method: total flavonoids are obtained according to chapter four of technical Specification 2003 edition for health food inspection and evaluation.
3.4 evaluation index
Sterilizing the fructus Rosae Normalis raw juice by high temperature sterilization and non-thermal sterilization, and detecting the contents of VC, SOD and flavone in the sterilized fructus Rosae Normalis pure juice.
3.5 Committee China inspection and quarantine science research institute comprehensive detection center to detect
Report number: CAIQS002000391300407.
4. Statistical analysis
The experimental data are expressed as means ± SD, and the statistical analysis is performed by means of two-sample mean t-test between groups for each index, with p × < 0.05, p × < 0.01, p × < 0.001, and the significance is poor, using statistical software "clinician statistical assistant V10.0".
6. Results of the experiment
TABLE 4 data of VC, SOD and flavone
TABLE 5 average number of VC, SOD and flavone groups
As can be seen from tables 5 and 6, the data of VC and flavone are reduced in the two indexes, i.e. VC and flavone are damaged to different degrees in any sterilization method, but the damaged degree is larger in the 2 groups of heat sterilization methods, VC and flavone are reduced by 50.49% and 49.17% in the 2 groups of heat sterilization methods, respectively, and p values are less than 0.001 in the 1 group, and the difference is significant; although the non-thermal high-pressure sterilization investigation group 3 is damaged, VC and flavone are respectively reduced by 3.38 percent and 4.17 percent, the p value is larger than 0.05, and the difference is not significant, namely the non-thermal sterilization VC and the flavone have the minimum damage, so the method is the best sterilization method and the difference is not significant.
Compared with the non-heat sterilization of the group 3, the degree of the VC and the flavone in the group 2 is much larger, the p values are both less than 0.001, and the difference is significant.
TABLE 6 comparison of data for VC, SOD and flavone
As can be seen from tables 5 and 6, the SOD in the group 2 was reduced by 30.36% and the damage degree of SOD was larger, the p-value was less than 0.001, and the difference was significant, compared with the group 1.
As can be seen from tables 5 and 6, the SOD of the non-autoclave sterilization group 3 was not reduced but increased by 56.98% compared with the group 1, and the difference was significant; compared with the heat sterilization 2 group, the SOD in the non-heat high-pressure sterilization 3 group is higher by 125.41 percent, and the difference is significant.
The purpose of autoclaving is to kill harmful bacteria and inactivate (inhibit) the activity of enzymes, thereby preventing fermentation, putrefaction and deterioration of foods, fruit juices, etc.
In the world and at home, the reason is that the original juice of the roxburgh rose is not sterilized under heat and high pressure for the first time, the SOD is not damaged, and the active content of the SOD in the pure juice of the roxburgh rose is improved.
In the actual product detection, the active content of SOD can break through 10000u/g and reach 12500u/g at many times, the forming mechanism is not clear, but theoretically, the following reasons should be found:
(1) by autoclaving, the cell wall is broken under high pressure and SOD present in the cells is released.
(2) Two subunits of copper and zinc of superoxide dismutase (Cu/Zn SOD) form coordinate bonds with a histidine side chain on an active site, and are mainly combined together through hydrophobic and electrostatic interaction, and the SOD activity is not generated when the hydrophobic and electrostatic interaction is not enough to combine the subunits of copper and zinc of superoxide dismutase; the SOD is combined under the action of pressure, and then the SOD has SOD activity and is released. The active sites of Mn SOD and Fe SOD have the same type of amino acid coordinated with metal ions.
(3) There are free protein components or fragments or short chain proteins and metal ions inside or outside the cell, which are in a free state in normal juice or pulp, making them possible to bind when subjected to pressure.
7. Conclusion of the experiment
From the above experiments, the VC, SOD and flavone are largely destroyed by heating and sterilizing the roxburgh rose juice, but the VC and flavone are hardly destroyed by non-heating and high-pressure sterilization and can activate the activity of SOD in the roxburgh rose juice.
Experiment three:
the microbial detection experiment of the freeze-dried powder prepared by sterilizing and non-sterilizing the roxburgh rose pure juice.
1. Purpose of the experiment
And (4) inspecting the microbial index condition of the freeze-dried powder prepared by sterilizing and non-sterilizing the roxburgh rose pure juice.
2. Test article
2.1 sterilizing lyophilized powder or analytical dried product of fructus Rosae Normalis pure juice
According to the method of the embodiment 1, the roxburgh rose is processed by juicing, filtering, non-heat sterilization, large package cleaning and disinfection, quick freezing, vacuum sublimation drying and vacuum desorption drying to prepare a sterilization desorption dried product or freeze-dried powder.
2.2 non-bactericidal lyophilized powder or analytical dried product of fructus Rosae Normalis pure juice
According to the method of example 1, fructus Rosae Normalis is subjected to juicing, filtering, (without non-heat sterilization), cleaning and sterilizing in large package, rapidly freezing, vacuum sublimation drying, and vacuum desorption drying to obtain non-sterilization desorption dried product or lyophilized powder.
3. Experimental methods
3.1 sampling Rosa roxburghii Tratt pure juice sterilization freeze-dried powder and Rosa roxburghii Tratt pure juice non-sterilization freeze-dried powder respectively, and respectively editing No. 1 and No. 2, and making two parts in parallel.
3.2 measurement method
The pathogenic bacteria include salmonella, shigella, and staphylococcus aureus, and are determined according to the method specified in GB/T4789.21.
3.3 measurement of indices
Respectively measuring microbial indexes of the roxburgh rose pure juice non-sterilization freeze-dried powder and the roxburgh rose pure juice sterilization freeze-dried powder, wherein pathogenic bacteria comprise salmonella, shigella and staphylococcus aureus.
4. Measurement results
The results of the microbiological assay of the sterilized lyophilized powder of fructus Rosae Normalis and the non-sterilized lyophilized powder of fructus Rosae Normalis are shown in Table 7 below.
TABLE 7
| Numbering | Salmonella | Shigella | Staphylococcus aureus |
| 1 | Not detected out | Not detected out | Not detected out |
| 2 | Detect out | Detect out | Detect out |
| 1′ | Not detected out | Undetected | Not detected out |
| 2′ | Detect out | Detect out | Detect out |
From the measurement results in the table 7, pathogenic bacteria are not detected in all the roxburgh rose sterilization freeze-dried powder, and pathogenic bacteria are detected in all the roxburgh rose freeze-dried powder which is not sterilized, which indicates the importance of the freeze-dried powder in the previous process sterilization. The fresh roxburgh rose fruit can carry bacteria and can be polluted in the processes of transportation, cleaning, juicing and filtering, so that the fresh roxburgh rose fruit serving as food needs to adopt a sterilization process to ensure the quality and safety of the product to ensure that the product has no pathogenic bacteria.
Experiment four:
rosa roxburghii freeze-dried powder and Rosa roxburghii biological preparation deliquescence experiment
1. Experimental methods
According to the methods of example 1, example 2 and example 3, coated tablets, uncoated tablets and granules of non-heat sterilization analysis dry products, namely roxburgh rose freeze-dried powder and roxburgh rose biological freeze-dried preparation, are respectively prepared.
Respectively spreading the prepared roxburgh rose freeze-dried powder (non-heat sterilization analysis dry product) and appropriate amount of unpacked roxburgh rose biological freeze-dried preparation coated tablets, non-coated tablets and granules, namely bare tablets on paper, standing for 30 days in an environment with room temperature RH75%, and observing the appearance condition of the tested product every 3 days. The test article is easy to absorb moisture (+++), when melted and deformed and adhered together; the tested product is moist, insoluble and deformable and is easy to absorb moisture (++); the slight tide of the test article is (+); the sample does not see a change of the score of one.
2. Results of the experiment
TABLE 8 Dequescence test of fructus Rosae Normalis lyophilized powder and fructus Rosae Normalis biological preparation
| Serial number | Observation time | Freeze-dried powder | Coated tablet | Non-coated tablet | Granules | Remarks for note |
| 1 | Day 3 | + | - | - | - | - |
| 2 | Day 6 | ++ | - | - | - | - |
| 3 | Day 9 | +++ | - | - | - | - |
| 4 | Day 12 | Complete liquefaction | - | - | - | - |
| 5 | Day 15 | Complete liquefaction | - | - | - | - |
| 6 | Day 18 | Complete liquefaction | - | - | - | - |
| 7 | Day 21 | Complete liquefaction | - | - | - | - |
| 8 | Day 24 | Complete liquefaction | - | - | - | - |
| 9 | Day 27 | Complete liquefaction | - | - | - | - |
| 10 | |
Complete liquefaction | - | - | - | - |
As can be seen from Table 8, the non-heat sterilized desorption dry product, i.e., lyophilized powder, absorbed moisture slightly on day 3; absorbing moisture on day 6, but not melting and deforming; absorbing moisture on the 9 th day, melting, deforming and adhering together; completely liquefied by day 12. While the coated tablets, uncoated tablets, granules of the pear biological lyophilized preparation showed no change in appearance on day 30.
It is demonstrated that in industrial production, the non-heat sterilization desorption dry product, i.e. freeze-dried powder, is not subjected to subsequent mixing with proper auxiliary materials, granules are subjected to granulation and microencapsulation, or tablets are subjected to industrial process treatments such as granulation, tabletting, coating and the like, humidity control and moisture absorption prevention, and the stability of the quality of the granules is difficult to guarantee. The coated tablet, the non-coated tablet and the granule of the pear biological freeze-dried preparation are mixed with proper auxiliary materials in advance and are treated by industrial processes of granulation, microencapsulation, tabletting, coating and the like, such as moisture control and moisture absorption prevention, so that the stability of the quality of the pear biological freeze-dried preparation is well ensured.
Experiment five:
determination of critical relative humidity of roxburgh rose biological freeze-dried preparation
1. Purpose of experiment
The critical relative humidity of the coated tablet, the non-coated tablet and the granules of the rosa roxburghii biological freeze-dried preparation prepared by the technical scheme is measured to ensure the product quality.
2. Test article
The method of example 1, example 2 and example 3 are respectively followed to prepare coated tablets, uncoated tablets and granules of the roxburgh rose biological freeze-dried preparation.
3. Experimental methods
Respectively drying appropriate amounts of the prepared coated tablets, the prepared non-coated tablets and the prepared granules of the biological freeze-dried preparation of the roxburgh rose to constant weight, respectively and uniformly placing the coated tablets, the prepared non-coated tablets and the prepared granules with the thickness of about 2mm at the bottom of a flat weighing bottle with the constant weight, accurately weighing, respectively placing the tablets, the prepared non-coated tablets and the prepared granules into dryers of supersaturated solutions of 8 different salts with different RH percent, keeping the solutions at room temperature for 7 days, and then weighing. Since ambient humidity has a great influence on coated tablets, uncoated tablets and granules, the critical relative humidity of coated tablets, uncoated tablets and granules was determined for this purpose.
Supersaturated solutions of different salts are prepared according to the table 9, the supersaturated solutions are respectively placed in a glass dryer, the supersaturated solutions are placed at room temperature for 48 hours, the internal humidity of the supersaturated solutions is balanced to form environments with different relative humidity, 2 tablets of each coated tablet and uncoated tablet which are dried to constant weight, 1.20g of the coated tablet and 1.00g of the granules are placed in flat weighing bottles with constant weight, the weighing bottle caps are precisely weighed, the coated tablets and the uncoated tablets are placed in the dryers with different humidity, the coated tablets and the uncoated tablets absorb moisture to constant weight at constant temperature, the moisture absorption rate is precisely weighed, 2 parts are parallelly prepared, and the results of measuring the Critical Relative Humidity (CRH) are respectively shown in tables 10, 11 and 12 and figures 2, 3 and 4.
TABLE 9 relative humidity of saturated solutions of different salts at 25 deg.C
TABLE 10 critical RH measurement data for coated tablets
| Number RH | 22.45 | 33.00 | 42.76 | 57.70 | 75.28 | 84.26 | 92.48 | 100.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 1 weight of water (g) | 0.00 | 0.01 | 0.03 | 0.07 | 0.22 | 0.43 | 0.74 | 0.96 |
| Water absorption (%) | 0.00 | 0.83 | 2.50 | 5.83 | 18.33 | 35.83 | 61.67 | 80.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 2 weight of water (g) | 0.00 | 0.02 | 0.04 | 0.08 | 0.20 | 0.44 | 0.76 | 0.94 |
| Water absorption (%) | 0.00 | 1.67 | 3.33 | 6.67 | 16.67 | 36.67 | 63.33 | 78.33 |
| Average Water absorption (%) | 0.00 | 1.25 | 2.92 | 6.25 | 17.50 | 36.25 | 62.50 | 79.17 |
TABLE 11 Critical relative humidity measurement data for uncoated tablets
| Number RH | 22.45 | 33.00 | 42.76 | 57.70 | 75.28 | 84.26 | 92.48 | 100.00 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 1 weight of water (g) | 0.00 | 0.02 | 0.04 | 0.08 | 0.23 | 0.44 | 0.76 | 1.00 |
| Water absorption (%) | 0.00 | 1.67 | 3.33 | 6.67 | 19.17 | 36.67 | 63.33 | 83.33 |
| Tablet weight (g) | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 |
| 2 weight of water (g) | 0.00 | 0.01 | 0.03 | 0.08 | 0.24 | 0.45 | 0.77 | 0.95 |
| Water absorption (%) | 0.00 | 0.83 | 2.50 | 6.67 | 20.00 | 37.50 | 64.17 | 79.17 |
| Average Water absorption (%) | 0.00 | 1.25 | 2.92 | 6.67 | 19.58 | 37.08 | 63.75 | 81.25 |
TABLE 12 measurement of critical relative humidity of granules
4. Analysis of results
The moisture absorption or water absorption percentage% in tables 10, 11, and 12 are plotted as ordinate and relative humidity RH% as abscissa, respectively, and the tangents at both ends of the curve are plotted, and the abscissa corresponding to the intersection of the two tangents is the critical relative humidity, to obtain fig. 2, fig. 3, and fig. 4. According to the experimental items, the critical relative humidity CRH of the coated tablets, the non-coated tablets and the granules of the roxburgh rose biological freeze-dried preparations is 74.92%, 72.41% and 72.37%, respectively, namely the environmental humidity of the coated tablets, the non-coated tablets and the granules of the roxburgh rose biological freeze-dried preparations is controlled to be below 72% and 74% during packaging, storage, transportation and the like so as to reduce the influence of moisture on the properties and stability of the coated tablets, the non-coated tablets and the granules of the roxburgh rose biological freeze-dried preparations.
From the above experiments, the critical relative humidity CRH of the coated tablet, the non-coated tablet and the granule of the biological freeze-dried preparation of rosa roxburghii tratt is 74.92%, 72.41% and 72.37%, respectively, which is only the critical relative humidity of the coated tablet, the non-coated tablet and the granule in the case of bare tablet, for example, after the coated tablet and the non-coated tablet are packaged by aluminum plastic blister or aseptic bagging or bottled and aseptic packaging of the granule, the critical relative humidity is higher, the shelf life is longer, and the stability of the product is further ensured.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. The preparation method of the rosa roxburghii biological freeze-dried preparation is characterized by comprising the following steps: carrying out non-thermal sterilization treatment on the roxburgh rose pure juice by adopting ultrahigh pressure, quickly freezing the sterile roxburgh rose pure juice, carrying out vacuum sublimation drying and vacuum desorption drying treatment in sequence in a low-temperature environment, mixing the roxburgh rose pure juice and auxiliary materials into a mixed material, and then preparing the mixed material into tablets, granules, powder or capsules according to actual conditions to obtain the roxburgh rose biological freeze-dried preparation.
2. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 1, which is characterized in that: the granules are prepared by granulating, microencapsulating and aseptically packaging the mixed materials; the tablet is prepared by granulating, tabletting, coating, aluminum-plastic bubble cap or aseptic bagging or bottling the mixture.
3. The preparation method of the biological freeze-dried roxburgh rose preparation according to claim 1 or 2, which is characterized by comprising the following steps:
(1) Pretreatment: cleaning fresh Rosa roxburghii Tratt fruit and air drying surface water for use;
(2) Juicing: feeding the fresh roxburgh rose fruits processed in the step (1) into a juicer to carry out juicing, and filtering and removing residues twice to obtain pure roxburgh rose juice;
(3) Non-thermal sterilization treatment: sealing the roxburgh rose pure juice in the step (2) by using a large packaging plastic bag or a plastic bottle, then sending the plastic bag or the plastic bottle filled with the roxburgh rose pure juice into a high-pressure cabin of an ultrahigh-pressure container, adding a medium, then sealing the high-pressure cabin, applying pressure to the ultrahigh-pressure container, maintaining the pressure and sterilizing to obtain sterile roxburgh rose pure juice;
(4) Cleaning and disinfecting a large package: conveying the sterilized roxburgh rose pure juice large package obtained in the step (3) to a sterile environment through a clean air curtain for cleaning, sterilizing and disinfecting; the big package is a plastic soft package or is filled in a plastic bottle;
(5) Quick freezing: under the aseptic environment, unpacking the large package cleaned and disinfected in the step (4), subpackaging the aseptic roxburgh rose pure juice into bracket layered trays, and sending the tray into a quick freezing warehouse or a freeze dryer for quick freezing to obtain frozen roxburgh rose pure juice;
(6) Vacuum sublimation drying: conveying the frozen pure roxburgh rose support layered tray obtained in the step (5) into a sublimation drying chamber for vacuum sublimation drying, so that frozen water molecules are directly sublimated into water vapor to be removed, and thus obtaining a sterilized freeze-dried pure roxburgh rose product, namely a vacuum sublimation dried product;
(7) Vacuum analysis and drying: collecting the vacuum sublimation dried product, respectively placing the collected vacuum sublimation dried product and the auxiliary material into a bracket layered tray, sending the bracket layered tray and the auxiliary material into a vacuum analysis drying chamber for vacuum analysis drying, and evaporating part of water remained in the sublimation freeze-dried product and the auxiliary material to obtain a real-fast analysis dried product and a dry auxiliary material;
(8) Mixing: according to the weight portion ratio, stirring, mixing and homogenizing the vacuum analysis dried product and the dry auxiliary materials at a certain rotating speed, and preparing tablets, granules, powder or capsules according to actual conditions to obtain the biological freeze-dried preparation of the roxburgh rose.
4. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: in the step (2), the filter screen for the first filtration is 200-300 meshes, and the filter screen for the second filtration is 400-800 meshes.
5. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, wherein the method comprises the following steps: in the step (3), the medium is water or high-grade hydraulic oil; when the medium in the ultrahigh pressure container is water, applying 400-600 MPa of pressure to the roxburgh rose pure juice packaged by a plastic bag or a plastic bottle, and keeping the pressure for 5-15 min; when the medium in the ultrahigh pressure container is high-grade hydraulic oil, applying pressure of 100-1000 MPa to the roxburgh rose pure juice packaged by a plastic bag or a plastic bottle; the pressure maintaining time is 1-30 min.
6. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: in the step (5), the temperature of the quick freezing is-30 to-40 ℃.
7. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: in the step (6), the vacuum degree of the vacuum sublimation drying is 30-150 pa, the temperature is 30-40 ℃, and the water content of the vacuum sublimation dried product is 10 +/-2%.
8. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: in the step (7), the vacuum degree of the vacuum analysis drying is 5-30 pa, the temperature is 40-60 ℃, the relative humidity of air is 20-40%, and the water content of the real fast analysis drying product is 5 +/-2%; the auxiliary materials are mixed auxiliary materials prepared by mixing microcrystalline cellulose, micro-powder silica gel and dextrin according to the mass ratio of = (0.3-0.4): 0.2-0.4), and the mass ratio of the microcrystalline cellulose, the micro-powder silica gel and the dextrin is 1.
9. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: in the step (8), the mass ratio of the vacuum analysis dried product to the drying auxiliary material =1 x, and x is less than or equal to 1; the rotating speed is 500-600 r/min.
10. The method for preparing the biological freeze-dried roxburgh rose preparation according to claim 3, which is characterized in that: the content of VC in the roxburgh rose biological freeze-dried preparation is more than or equal to 30mg/g, the content of SOD biological activity is more than or equal to 20000-50000 u/g, and the content of flavone is more than or equal to 4mg/g; pathogenic bacteria, namely salmonella, shigella and staphylococcus aureus, are not detected in the roxburgh rose biological freeze-dried preparation; the critical relative humidity of the rosa roxburghii tratt biological freeze-dried preparation is more than or equal to 70 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210737030.5A CN115349613B (en) | 2022-08-31 | 2022-08-31 | Preparation method of roxburgh rose biological freeze-dried preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210737030.5A CN115349613B (en) | 2022-08-31 | 2022-08-31 | Preparation method of roxburgh rose biological freeze-dried preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115349613A true CN115349613A (en) | 2022-11-18 |
| CN115349613B CN115349613B (en) | 2023-08-18 |
Family
ID=84030105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210737030.5A Active CN115349613B (en) | 2022-08-31 | 2022-08-31 | Preparation method of roxburgh rose biological freeze-dried preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115349613B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116076680A (en) * | 2023-01-10 | 2023-05-09 | 华南理工大学 | Rosa roxburghii spray powder rich in bioactive components and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105360277A (en) * | 2015-12-03 | 2016-03-02 | 贵州华南理工生物工程有限公司 | Superhigh-pressure fresh keeping method for fresh rosa roxburghii |
| CN106036604A (en) * | 2016-05-26 | 2016-10-26 | 安顺职业技术学院 | Vacuum freeze-drying processing technology of rosa sterilis fruits |
| CN107535787A (en) * | 2016-06-23 | 2018-01-05 | 上海蓝王医药科技发展有限公司 | A kind of Rosa roxburghii freezes the preparation method of particle |
| CN110140909A (en) * | 2019-05-30 | 2019-08-20 | 重庆康菌泰生物科技股份有限公司 | A kind of Rosa roxburghii Tratt comprehensive enzyme and preparation method thereof |
| CN111265657A (en) * | 2020-02-26 | 2020-06-12 | 中国农业大学 | Superoxide dismutase solid preparation and preparation method thereof |
| CN112006191A (en) * | 2020-07-27 | 2020-12-01 | 遵义师范学院 | Roxburgh rose fruit juice beverage and preparation method thereof |
-
2022
- 2022-08-31 CN CN202210737030.5A patent/CN115349613B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105360277A (en) * | 2015-12-03 | 2016-03-02 | 贵州华南理工生物工程有限公司 | Superhigh-pressure fresh keeping method for fresh rosa roxburghii |
| CN106036604A (en) * | 2016-05-26 | 2016-10-26 | 安顺职业技术学院 | Vacuum freeze-drying processing technology of rosa sterilis fruits |
| CN107535787A (en) * | 2016-06-23 | 2018-01-05 | 上海蓝王医药科技发展有限公司 | A kind of Rosa roxburghii freezes the preparation method of particle |
| CN110140909A (en) * | 2019-05-30 | 2019-08-20 | 重庆康菌泰生物科技股份有限公司 | A kind of Rosa roxburghii Tratt comprehensive enzyme and preparation method thereof |
| CN111265657A (en) * | 2020-02-26 | 2020-06-12 | 中国农业大学 | Superoxide dismutase solid preparation and preparation method thereof |
| CN112006191A (en) * | 2020-07-27 | 2020-12-01 | 遵义师范学院 | Roxburgh rose fruit juice beverage and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116076680A (en) * | 2023-01-10 | 2023-05-09 | 华南理工大学 | Rosa roxburghii spray powder rich in bioactive components and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115349613B (en) | 2023-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2925300B1 (en) | Microparticles comprising a probiotic, cross-linkable reagent, a denatured protein, polyol plasticiser and trehalose | |
| Jiang et al. | Fruit and vegetable powders | |
| US20070160700A1 (en) | Methods and compositions for reactivating acetylcholinesterase | |
| CN115349613B (en) | Preparation method of roxburgh rose biological freeze-dried preparation | |
| CN103053738A (en) | Tea-processing herba cistanche and preparation method thereof | |
| CN109105889A (en) | A kind of preparation process and application of the Rosa roxburghi Juice that ferments | |
| CN107594109A (en) | A kind of pet drinks enzyme liquid and preparation method thereof | |
| CN103844251B (en) | Super micro-pueraria root powder, agate flower health care particle and its production and use | |
| CN101919567B (en) | Wheat malt drink and production method thereof | |
| Petzold et al. | Food technology approaches for improvement of organoleptic properties through preservation and enrichment of bioactive compounds | |
| CN111374246A (en) | Method for producing lycium ruthenicum juice by utilizing ultrahigh pressure technology | |
| CN106360207B (en) | Method for preparing chitosan oligosaccharide maca ginseng functional beverage and functional beverage prepared by same | |
| CN109077320A (en) | The chewable tablets and preparation method thereof of phenolic substances in a kind of absorption blueberry residue | |
| CN106942728B (en) | A kind of clover barley product and its preparation method and application | |
| CN104172154A (en) | Wild vegetable tea powder and preparation method thereof | |
| CN109219358A (en) | For reducing the edible composition of nocuousness/toxicant digestibility or absorptivity | |
| JP2006256969A (en) | Blood flow ameliorant | |
| JP2010537670A (en) | Morinda citrifolia preparation for regulating T cell immune regulation in newborn livestock | |
| JP2006008645A (en) | Method for producing extract of inonotus obliquus | |
| KR101171846B1 (en) | Post-harvest Amplification Method of Active Compounds in Brassicaceae Vegetables Using High Hydrostatic Pressure and Brassicaceae Vegetables Treated with the Same Method | |
| CN1098094C (en) | Preparation process of fresh animal and plant superactivity protoplasm | |
| CN109007518A (en) | A kind of low temperature integration processing method of seabuckthorn fruit powder and its application | |
| CN110419717A (en) | A kind of preparation method avoiding viscous wall and the ganoderma spove powder for delaying oxidation | |
| CN113907234B (en) | Rhizoma polygonati primary pulp and preparation method thereof | |
| CN114129648A (en) | Extraction method of high-purification aloe dry powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |